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Acetic Acid → HCID 70137322, 화합물

HRID 367329
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HRID 367329 반응식
C(OC([NH:11][C@H:12]1[CH2:21][CH2:20][C:19]2[C:14](=[CH:15][C:16]([O:22][CH2:23][C:24]([N:26]([CH3:28])[CH3:27])=[O:25])=[CH:17][CH:18]=2)[CH2:13]1)=O)C1C=CC=CC=1.[H][H].[C:31]([OH:34])(=[O:33])[CH3:32]>[C].[Pd]>[C:31]([OH:34])(=[O:33])[CH3:32].[NH2:11][C@H:12]1[CH2:21][CH2:20][C:19]2[C:14](=[CH:15][C:16]([O:22][CH2:23][C:24]([N:26]([CH3:28])[CH3:27])=[O:25])=[CH:17][CH:18]=2)[CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 53809809HCID 53809809, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 70137322HCID 70137322, 화합물

시약·촉매·용매 1

HCID 178418390HCID 178418390, 화합물촉매

실험 절차

(S)-2 -[2-(Benzyloxycarbonylamino)-1,2,3,4-tetrahydronaphthalen-7-yloxy]-N,N-dimethylacetamide (100 mg) and 20 mg of 10% palladium-carbon were suspended in 5 ml of acetic acid and the suspension was stirred at room temperature for 3 hours in an atmosphere of hydrogen. The catalyst was removed by filtration, the filtrate was concentrated under reduced pressure, and the residue was recrystallized from ethanoldiethyl ether to give 72 mg of (S)-2-(2-amino-1,2,3,4-tetrahydronaphthalen-7-yloxy)-N,N-dimethylacetamide acetate having a melting point of 135 to 142° C.

후처리

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customthe residue was recrystallized from ethanoldiethyl ether

출처 및 근거

ORD 기록
ord-7d48ca9d3f5a4935a1491ee77f613d45
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06133266

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